Apparatus for and method of distillation



Jan. 25, 1944. R. v. KLEINSCHMIDT 2,339,362

APPARATUS FOR AND METHOD OF DISTILLATION med Dec. 2:5, 1940 'INVENTOR ATTORNEYS Patented Jan. 25, 1944 2,389,862 APPARATUS FOR AND METHOD OF DISTILLATI N Robert V. Kieinschmidt,

signer to Arthur D. Mass, a corporation Little, 1110.,

Stoneham, Mass, as-

Cambridge,

Massachusetts Application December 23, 1940, Serial No. 371,298

1'7 Claims.

This invention relates to improvements in apparatus for and method of separating components of a fluid mixture of two or more substances by reason of their difference in boiling point or volatility. More particularly, my apparatus and erocess are applicable to those cases where both the initial mixture and the separated components are liquids during some portion of the process, but these liquids may be more or less concentrated solutions of solids, liquids or gases in liquids or liquid mixtures of materials normally in solid or gaseous form in the pure state. My apparatus and process relate generally to what is commonly referred to as distillation, fractionation, rectification, evaporation, concentration, and the like, which are characterized by the evaporation of a portion of a liquid mixture. Any such liquid mixture is referred to herein as a solution, and any such operation is referred to herein as distillation, for purposes of brevity.

It is a purpose of the present invention to iacilitate the control of a distillation operation wherein vapors evolved from a solution are compressed and brought into out-oi-contact heat exchange relation with solution in a vaporization chamber or zone so that energy of compression may beutilized in causing further solution to be evaporated and thereby maintain a continuous process. In carrying out such an operation, the compressed vapor, which is condensed in heat exchange with boiling solution, results in a condensate which is taken from the system, preferably in counterflow heat exchange relation with the solution entering the system, so as to preheat the solution in a preheating chamber or zone before it enters the vaporization zone.

In my Patents Nos. 2,185,595 and 2,185,596, I have described a distillation method and apparatus which can be operated continuously under constant conditions such as rate of distillation, amount and concentration of overflow, pressure on the feed valve, and efliciency heat transfer surfaces. If it. is desired to operate such appa? ratus under another set of conditions, it will normally be necessary to readjust the apparatus until desired operation is attained. This is due in part to the'fact that there is a tendency for the portion of the heat exchanger tube which is condensing vapor to vary with the amount of vapor being condensed. The result is that at high rates of distillation there may be insui'licient tubing left in the preheater zone to preheat the feed and cool the condensateto desired degree.

In the present invention, I have provided means whereby the condensing section can sharply limited in length and the relations of flow, pressure drop and condensing surface are adjusted in the design and construction of the apparatus to automatically adjust the rate of condensation over a range of distillation rates. Moreover, I have provided feed control means that will automatically supply the correct predetermined amount of feed at all rates of distillation. In this way, I am. able to provide a complete self-regulating system of distillation, which, in addition to requiring less attention durin normal constant operation, permits a range of rates of distillation, while maintaining desired distillation conditions, merely upon varying the amount by weight of liquid in vapor ,form that is compressed by the compressor.

It is a feature of this invention that the rate of condensation of compressed vapor which is brought into out-of-contact heat exchange with solution in the vaporization zone is automatically controlled upon variation in the capacity of the compressor to discharge vapor under pressure relatively to the capacity of the condenser to condense the vapors at a given temperature difierentlal between the condensing compressed vapors and the boiling solution in the vaporization zone. This automatic control may be effected, according to this invention, by causing the condensate resulting from condensation of the compressed vapor to flow through an orifice of limited cross-section, which has the effect or increasing the pressure on the uncondensed vapor undergoing condensation whenever the amount of compressed vapor discharged by the compress01 is increased. In this manner, the temperature diiierential between the compressed vapor in the condenser and the boiling solution in the vaporization zone is increased, until the rate of condensation of the vapor is increased suificient- 1y to take care of the increased amount of vapor discharged by the compressor. It is to be noted that this is accomplished without materially changing the extent 0! the condensation zone in the apparatus. Any vapor which reaches the restricted orifice, being oi! much greater volume than the condensate, acts with a throttling action at the orifice so as to build up the pressure on the condenser side of the orifice, with the result above described. I

It is a further feature 01 this invention that the rate oi feeding solution to be distilled into the apparatus is automatically varied, dependin! upon the amount of vapor handled by the compressor, so that the capacity or the distillation unit can be varied merely by changing the 2 aaaaaes capacity of the compressor and without need for manually adjusting the rate of feed once the desired conditions of the distillation operation are observed to have been established. This may be accomplished by actuating the compressor by 6 suitable means and controlling the rate of feed by a pump or equivalent device by means coacting with means for varying the output of the compressor, so that whenever the output of the com ressor is varied, the rate of feed supply is 10 varied substantially proportionally.

Further features of this invention relate to the co-operation between the automatic control of the capacity of the condenser and of the rate of the feed, so that the distillation unit is fully automatic in all respects. Other features of this invention relate to supplemental means for controlling the rate of feed in a manner which is useful during the starting of the apparatus.

Further purposes, features and advantages of this invention will be apparent in connection with the following description of the illustrative embodiments of this invention which are shown in the accompanying drawing, wherein Figure l is a side elevational view, principally schematic, of a simple type of apparatus embodying this invention;

Fig. 2 is a side elevational view, partially in section and partially schematic. of a form of apparatus embodying this invention which is typical of apparatus appropriate for commercial installation: and

Fig. 3 is a side eievational view partially schematic of a modified means for proportionally controlling the output of the compressor and pump in the system shown in Fig. 2.

Referring to Fig. l, the distillation apparatus comprises a shell 10 into which solution to be distilled is introduced by line II that enters the shell "I adjacent the bottom thereof. The solution i2 to be distilled may be contained in a reservoir I! from which it can be pumped by pump I through line l5 having a mouth adjacent the bottom of reservoir ll. In this manner, the solution to be distilled is taken from the reservoir I3 and fed into the bottom of the shell III at a rate which is controlled by the rate of operation of the pump H. The pump i4 is preferably of a positive displacement type so that the rate of feed may be controlled as accurately as possible depending upon the rate of operation of the pump. At the top of the shell i0 is a vapor separator I from which vapor is taken by line ll to the compressor 18, which may be of any suitable type suchas a piston type compressor or a rotary compressor: e. g.. a rotary compressor of the Roots Connersviile type. Preferably the compressor is of a positive displacement type so that the amount by weight per unit of time of liquid in vapor form compressed by the compressor may be controlled as accurately as possible, depending upon the rate of operation of the compressor. In the compressor it the vapor is compressed to a pressure such that its condensing temperature is above the boiling point of solution to be vac5 porized in the upper portion of the shell Ill. The

compressed vapor is discharged from the compressor by line I! and enters the condenser heat exchanger 20 in out-of-contact heat exchange with solution within the shell Ill. Adjacent the lower portion of the condenser 20 is a restricted orifice 2i, the purpose and operation of which will be described more in detail hereinbeiow. In order to withdraw condensate resulting from com densation of vapor in the condenser 20, the line 22 is provided, which acts as a cooling heat exchanger and which directs the outflowing condensate in counterflow heat exchange with solution introduced into the shell 20 through line H and serves to preheat the incoming solution in the lower preheater portion of the shell "I before the solution reaches the upper vaporization portion of the shell Ill. The normal liquid level in the distillation apparatus is determined by the level of overflow line 23, the mouth of which is slightly above the lower part of the vapor separator l6. The overflow line 23 preferably extends downwardly through the shell IG so that sensible heat of the withdrawn concentrated solution may be given up by heat exchange with incoming fresh solution, thereby increasing the efilciency of the system. In order to facilitate the starting of the apparatus, a by-pass line 24 controlled by valve 25 is provided, the by-pass line 21 preferably having an outlet adjacent the normal liquid level of liquid in the still, in the manner described more fully in my Patent No. 2,185,596 and which is exemplified herein by the outlets 28 that are slightly above the normal liquid level of solution in the still. In normal operation oi the device, the valve 25 is maintained in closed position.

The compressor I8 is operated by a motor 21 which drives the shaft 28. The rate of output or capacity of the compressor for compressing vapor is proportional to the speed of rotation of the shaft 28 driven by the motor 21. The compressor is operated from shaft 28 by any suitable operative actuating mechanism 29. The pump I 4 is also operated by the motor 21 through suitable positive connecting means such as the complementary conical pulleys 30 and 30' and belt 8i. By using conical pulleys 30 and 30' and belt 3|, the relative rate of operation of the compressor l8 and of the pump it can be adjusted as desired and can be maintained at any suitable setting. After the desired relative operation of the compressor I8 and the pump it has been determined, the setting of the belt 3| so as to maintain the desired rate of operation normally is maintained undisturbed during the distillation operation and during any change in the rate at which the distillation operation is carried on.

A by-pass line 32 leads from the feed line H so that solution discharged from the pump I 4 can be recirculated to the pump. If desired, solution by-passed through line 82 can be by-passed back to the reservoir i3 through line 33 controlled by valve 24. Alternatively, the solution by-passed through line 32 can be returned directly to the pump M by opening valve 35 and closing valve 34. In either event, the by-passed solution is to be regarded as being returned to the suction side of the pump II,

The operation of the distillation apparatus above described may be illustrated as follows. When it is desired to institute a distillation operation, the motor 21 is started, which simultaneously operates the compressor i8 and the pump II. Solution I2 is taken from the reservoir i3 and caused to flow into the shell ill until it starts to overflow from the overflow line 22. The valves 34 and 35 are then opened (either one or the other or both). so that the solution pumped by the pump I4 will be recycled and will not cause an excessive amount of undistllled solution to flow from the still through overflow line 28. If desired, the rate of flow in the feed line H may be controlled by the valve 36 so as to ensure the proper by-passing of the soluvalve 25 in that the amount tion pumped by the pump ii. at the same time, the valve II is opened so that gaseous fluid comprising air and vapor in the vapor separator It will be recycled by the compressor ll warmed and until the vapor content is increased so that the amount of condensing vapor is sufficient to bring the solution in the upper part of shell II to boiling temperature. When the amount of vapor in the gaseous fluid that is by the compressor is sufilcient to boil part of shell i and maintain a continuous distillation operation, the line 24 is closed and the valves 34 and I in the by-pass line 32 are also closed. The valve 36 in the feed line H is, of course. set in open position.

The rate of operation of the pump II, it not previously adjusted as a result of prior operation of the apparatus, may be adjusted so that the solution to be proper concentration before being discharged through the line 23. This can be done lusting the position of the belt ii on the con ical pulleys I0 and 30. When the belt 31 has the desired setting and distillation conditions for continuous operation have become established, it is apparent that the pump II will supply fresh solution to be distilled so by weight per unit of timefioi the solution will be proportional to the amount by weight per unit of time oi liquid in vapor form compressed by the compressor 18. While the rate of operation of the compressor Iii remains constant, the rate of feed will likewise the rate of feed will be appropriate for achieving the desired extent of concentration of solution being distilled. Ii, however. the rate of operation of the compressor is varied by varying the speed of the motor 21, the rate or teed will be automatically changed by the change in rate of operation of the pump ll while still maintaining substantially the same the amount by weight per unit of time of solution fed into the system by the pump and the amount by weight per unit of time ofliquid in vapor form compressed by the compressor. For example, if it is desired the still as a whole by ically introduced into the still so as to take care of the increased amount of vapor withdrawn from the vapor separator l6 and condensed in Ill, thereby maintaining the functloning oi the increased rate of output of the still. Conversely, ii the rate of operation of the compressor i0 is decreased, the rate of feed by pump ll will likewise be decreased automatically.

In the operation of the device, it is also pointed out that the capacity of the condenser I is varying the output or the still. This is accomplished by providing the restricted orifice 2| adjacent the lower part of the condenser 20. The orifice 2i automatically controls the capacity of the condenser 20 in the following manner.

During the operation of the apparatus, the

compressed by the compressor II is condense in the condenser Ill, part of the vapor ultimately the orifice II. The orifice ii is 0 sufficient size to pass the total amoimt of liq resulting from condensation of all the vapor cmn ressefl by the compressor.

However.

the device constant notwithstanding sure being greater the greater weight of liquid in permit more than a small amount 0! vapor to pass therethrough. This results from the tact that the volume or the vapor is many times the volume of the condensate. Due to the presence of the orifice II. the condensing vapor ten thereby in more than a very small amount. Depending upon the amount of which reaches the orifice II, the pressure condenser 20 is increased or decreased, the presthe amount 0! which reaches the orifice 2|. This results control, inasmuch as whenever the discharged from the compressor i8 is increased. the pressure in the condenser 20 is increased due to the throttling action of the orifice 2i, thereby increasing the temperature differential between the temperature of condensing liquid in the condenser 2|! and the temperature of the boiling liquid in the vaporization zone of the still. This greater temperature differential increases the rate of condensation until a sufiicient amount of the vapor is condensed so that all the condensate nearly free of vapor can pass through the orifice 2i. Conversely, if the rate 0! operation of the compressor is decreased, the pressure in the condenser III will fall, so that the rate of condensation becomes to permit condensate to pass through As aforesaid, some of the vapor passes through the orifice 2|, but the comes condensed in the region c just below the orifice ii in the vaporization zone. The condensation zone is indicated as a in the drawing and extends down through the vaporization zone or chamber of shell Ill and also takes in the region 0 just referred to. The condensate then passes down through the cooling heat exchanger which is in the preheating zone or chamber of the still, which is indicated as b.

The amount by weight of vapor which is permitted to pass the orifice 2| is very small and is usually less than two per cent oi the total vapor form compressed by the compresso Normally, the orifice is such that only about a fraction of one per cent oi the total weight of liquid in vapor form compressed by the compressor passes the orifice. operation, however, some of the uncondensed vapor reaches the orifice 2i and a small amount in the order above mentioned passes therethrough so that the variations in pressure of vapor on the compressor side of the orifice will be d in approximately proportional relation to the amo by weight per unit of time of liquid in vapor iorm compressed by the compressor notwithstanding variations in said amount compressed by the compressor and/or vapor in automatic amount of vapor variations in the capacity of the condenser to condense vapors in contact therewith. Alter any uncondensed vapor passes through the orifice, the pressure thereon and on condensate with which it is commingled is reduced and the residual vapor soon becomes condensed. When, lorexample. the outlet for the condensate is open tus self-regulatory. The rate of feed is regulated so as t of the apparatus. to be understood that the showing in Fig.

the most 1 is shown, the speed of which can be controlled by a rheostat 3 tor. Further in this connection, leys 3B and 30' speed-changing means may be erably, the speed-changing means that is used is centration of solution discharged tillation apparatus. With regard to the pump it, a positive displacement pump, preferably of the The motor 21 and indicated by similar refslmilar reference characters. rheostat 31 are likewise erence characters.

In Fig. 2, chamber 50 and a preheating chamber and the condenser tubes 56.

e motor 2'! drives the compressor 53 through the shaft 82, 82 that together with belt 3| for convenience in illustrating one type of speed-changing mechanism which may be employed.

Extending from the increase in power consumed. It will not be necessary to reduce the capacity of the unit.

While this invention has been described in connection with certain the light of invention. 10

the foregoing description of this I claim: 1. Distillation combination a apparatus which comprises in chamber adapted to contain a vaporization chambe 2. Distillation apparatus which comprises in combination a chamber adapted to contain a solution, a compressor adapted to compress a sion therein, heat exchange means arranged to maintain a fluid in out-oi'-contact heat xchange with solution in said chamber, means arranged for directing fluid comprmed by said oi time introduced into said Varying the common control means for chamber, rate of operation of said pump, and

controlling the tained in substantially the iation with the amount by of liquid in vapor form pressor.

compressor and said pump at predetermined relative peeds.

4. Distillation apparatus according to claim 2 wherein said means for introducing solution into said chambe valve-controlled bypass leading from the pressure side of said pump to the suction side of said pump.

5. Distillation apparatus according to claim 2 wherein said means for introducing solution into said chamber comprises a valve-controlled bypass leading from the pressure side of said pump to the suction side of said pump, and which inof said chamber level of liquid in p essed by said compressor to the amount by weight 01' solution introduced into said chamber remains substantially constant.

8. Distillation apparatus combination a chamber solution, a compressor adapted to compress a gaseous fluid containing vapor, means arranged for directing a gaseous fluid from the interior of said chamber into said compressor for compreselchange with solution in said chamber, preheater heat exchange means arranged to maintain a fluid in out-of-contact heat exchange with bolution to be distilled, means arranged for directing condensate resulting from heat exchange means, means arranged for introducing solution to be distilled into contact with said preheater heat exchange means and into said chamber including a pump arranged for controlling the amount by weight of ascasoa '7! solution per unit oi time introduced into said ll. Distillation apparatus according to claim bet, means for withdrawing concentrated 10 which comprises means including a restrictive solution from said chamber, common control orifice between said condenser heat exchange means for controlling the rate or operation or said means and said cooler heat exchange means for ranged so that the amount by weight of solution means and solution in said vaporization champcr unit time introduced into said chamber by her approximately in direct proportion to variathe action 0! said pump will be maintained in tions in the amount by weight of liquid in vapor the same proportional relation with form compressed by said compressor and ed the amount by weght per unit of time of liquid in to said condenser heat exchange means by varyvapor form compressed by said compressor, and lag the pressure or the vapor in said condenser means for varying the capacity or said condenser heat exchange means.

heat exchange means comprising an orifice which 12. A method of distillation which comprises is adjacent the outlet end or said condenser heat is feeding a solution to be distilled into and through exchange means, the cross-sectional area oi! a preheating zone and thence through a vaporizawhich is about Am o to yioo oo oi the heat transtlon zone, vaporizing a portion of said solution for surface of said condenser heat exchange in said vaporization zone, removing vapor evolved means, and which restricts the outlet or said from said solution in said va orization zone irom condenser heat exchange means so that upon go said vaporization zone, compressing the removed g the amount by weight per unit or time of vapor to a pressure at which the condensing temliquid in vapor form compressed by said compresperature is above the boiling point of solution sor from a first amount to a second amount the in said vaporization zone. supplying the comtemperature diflerential between the condensing pressed vapor in varying amount by weight per temperature of vapor in said condenser and the 5 unit of time to a condensation zone in out-oiboill g point of solution in said chamber will be contact heat exchange relation with solution in varied from first tem eratur din rn i t said vaporization zone thereby condensing vapor second temperature diflerential the ratio or which to a liquid. Withdrawing liquid fr ai ondenand sewnd te t r diflerentials being sation zone and passing it together with a small pproximately the same as the ratio of said first 3 amount or uncondenscd vapor to a cooling zone in a d second ammm out-oi-contact heat exchange with solution in ts l0. Disti lation apparatus which comprises a said oreheatingz n whil simlfl an u y rea va riz tion m m e ducing the pressure on said liquid in passing preheatin po means for introducing solution to be distilled into from s condensation zone to said cooling zone said preheating ch mber a d for directing if, to a pressure below condensation pressure but thence into said vaporization chamber, a comabove atmospheric Pressure wh e preventing the ressor for compressing vapor, a s arranged passage' of more an a small fraction of the {or ir ti v r from m vaporization chamvapor therewith. and then cooling the withber into said compressor for compression therei drown liquid nd m l ting condensation of condenser heat exchange means arranged to 40 \mcondenscd vapor in said cooling zone in outmgintain a, c nd n i Vapor m gutagj-gontact oi-contact heat exchange with solution in said heat exchange with solution in said vaporization P zonechamber, means ior directing compressed vapor A method according t c aim 12 wherein mpreggor d mm 4 condense;- the amount of solution per unit of time led into means in out-oi-contact heat ex- Sold preheating $0116 is varied P P Y W change with solution in said vaporization chamthe amount er unit or time compressed vapor her, a. cooler hea exchange meg, at anged supplied to said condensation zone. maintain liquid in out-oi-contact heat exchange A method of distillation h h c mpris with ol ti m i preheating chamber, means causing vapor to be evolved nimrom a solution in a arranged ior directing condensate resulting from 59 vaporization zonecomllrcis the evolved -P condensation oi vapor in said condenser heat Pr a W c exchan e means from said condenser heat ex We of the o en ing vapor is substantially i t id o e t x h above the boiling point of said solution, bringin out-oi-contaet heat exchange with s the compressed vapor into u -o o n5 heat exchange with said solution and comic cha m ranged to: withdrawing concentrated solution substantially of said va r whi in a he the one t or ini of va or porization zone. eedin iresh olution d by said compressor and supplied to said v p riz tion zone, t d aw s on nt e s condenser heat exchange means, positive" disto 111mm from said vaporization tone. on

acci ent reed control men to conthe emoun P t 0! d in vapor r trol amoun r t 01 time or solution in- @0111? said compressor y v troduced into said preheating chamb r, mo r -MW of h mpress r to compress vapor main positive displacement reed control means, and c5 al con tant a predetermined proportional reon drive means for said reed control means on b tw en th amount gar unit time or liqcom and said compress r operativeiv connected with 1115 in v p r f m compres by said com ress r said motor means and coactlng with said means and amount P91 tlmc of flesh Solution ior vanins the amount per unit or time of vapor fed i cold v p ri z n a h e mai com ress d by said compressor so that said To tain ns substantially constant a p e amount by weight per unit or time or liquid red rop onal relation between the amount per said'ieed control mean varies approximately un t time or liquid in vapor rorm co cl r by proportionally. with variations in the amount er said compressor and the pressur to which the unit or time by weight of liquid in vapor io m condensing vapor compressed by said compressor rested in said is is subjected. said predeterlnll 090M 8 assaaes relati nship between the amount per unit time per rea hing said strict ve rifice eing reduced oi liquid in vapor form com resse by said comin through said orifice. the condensation pressor and the p to which the condensin oi uncondensed vapor passing through said orifice vapor compressed by said compressorissubiected ing completed at a lower p and the main y easing said condensate to- 5 amount oi vapor passing through said restrictive ga her with uncondensed vapor through a restrlc cc at all es less than about two tive orifice which es a back p ssure upon per cent of the total weight of liquid in vapor uncondensed vapor between sai compressor and form compressed by the compressor d c at v depending upon the n a thod oi distillation wherein vapor amount or condensate and uncondensed vapor in is evolved irom a solution in a vaporization rea g said orifice, the ssure upon the unthe evolved vapor is compressed to a pressure at condensed vapor reach orifice being rewhich the condensing temperature is su tanduced in passing through said orifice. tialiy above the boiling point oi said solution in 15. In a method of distillation wherein vapor is said vaporization zon the compr ssed vapor is evolved from a solution in a vaporization zone. l condensed in out-oi-contact heat exchan e reto e densed in out-oi-contact heat exchange relation comprising passing condensed compressed vapor with said solution in said vaporization zone, fresh through a restrictive orifice located on the tar solution is introduced into said vaporization zone. side oi Said vaporization zone from said coniconcentrated solution is withdrawn from said pressor while passing a small amount of unconva orization zone. and condensate resulting irom densed compressed vapor through said orifice toeondensation of said compressed vapor is flowed gather with said condensate and maintaining the in-counterfiow out-oi-contaet heat exchan e rerate oi operation or said compressor within the lation in a preheating zone with fresh solution range wherein said restrictive orifice imposes entering said vaporization zone. the steps comback pressure between said orifice and said comprising the passing of condensate resulting from pressor at which the condensing temperature of the condensation oi said comp essed vapors 80 the compressed vapor is substantiall above the vapo exchan e surface at which condensing vapor is gether with condensate condensed in said vain out-oi-contact heat han relation with porization zone, thereby, causing said back preswhich the condensing temperature of said conrestrictive orifice and to correspondingly vary the densing vapor is substantially above the boiling temperature at which said com resse vapor conpoint or the solution in said vaporization zone denses prior to reaching said orifice, the p ssure liquid to rough said o co together with unfit-Kissing reduced in p ugh laid said condensate. thereby causing said back pres orifice.

vary depe ding upon the amount or con- 17. Amethod according to claim 16 wherein the densate and uncondensed vapor reaching said temperature difi'erential between the condensing restrictive orifice, and thereby co sin: to co revapor and the solution in the vaporization zone spondingly vary the temperature at which the is between about 5 1''. to about 1''.

said orifice, the p ssure upon uncondensed va- ROBERT v. mew. 

